FIELD: medicine.
SUBSTANCE: for quantitative determination of acetylsalicylic acid and its main salicylic acid metabolite in human plasma, liquid-liquid extraction of salicylates from the blood plasma is performed with subsequent derivatisation by silylating agent N-methyl-N-tret-butyldimethylsilyl-trifluoroacetamide. The analyzed compounds are determined by gas chromatographic mass spectrometry with an internal standard (p-toluic acid) on a non-polar HP-5MS capillary column at an injector temperature of 250°C and chromatograph oven initial temperature of 130°C. The column is thermostated for 2 minutes, and then heated to 280°C with a temperature gradient of 25°C/min. The column is then again thermostated at 280°C for 4 min. Mass spectra are recorded with "electron impact" ionisation at 70 EV and ion source temperature of 230°C. The recording of positive ions and scanning of selected ions with m/z 309 for acetylsalicylic acid and with m/z 195 for salicylic acid is performed in the monitoring mode at a rate of 2 scan/s.
EFFECT: invention provides pharmacokinetic drug monitoring in patients with cerebrovascular diseases.
9 dwg, 3 tbl, 1 ex
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Authors
Dates
2017-06-21—Published
2016-07-21—Filed